HRID641134

反应详情

EQUATION

反应方程式

HRID 641134 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2.6 g (11.2 mmol) Methyl-2-oxo-3-vinyl-1,2-dihydroquinoline-4-carboxylate 5 in 200 mL chloroform was added slowly over a dropping funnel a solution of 2.16 g (13.5 mmol) bromine in 15 mL chloroform and subsequently 6.8 mL of triethylamine. The reaction mixture was heated at reflux for 4.5 hour. After evaporation of the solvent the residue was purified by column chromatography on silica gel, eluting with toluene/ethyl acetate/methanol 4:1:1, to give 1.1 g of the desired product 6.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 4.5 hour
  3. customAfter evaporation of the solvent the residue
  4. customwas purified by column chromatography on silica gel
  5. washeluting with toluene/ethyl acetate/methanol 4:1:1